Multi-residue analysis of free and conjugated hormones and endocrine disruptors in rat testis by QuEChERS-based extraction and LC-MS/MS
Endocrine disrupting compounds (EDCs) are suspected to be responsible for many disorders of the human reproductive system. To establish a causality relationship between exposure to endocrine disruptors and disease, experiments on animals must be performed with improved or new analytical tools. There...
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| Veröffentlicht in: | Analytical and bioanalytical chemistry 2012-03, Vol.402 (9), p.2777-2788 |
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| creator | Pouech, Charlène Tournier, Mikaël Quignot, Nadia Kiss, Agneta Wiest, Laure Lafay, Florent Flament-Waton, Marie-Magdeleine Lemazurier, Emmanuel Cren-Olivé, Cécile |
| description | Endocrine disrupting compounds (EDCs) are suspected to be responsible for many disorders of the human reproductive system. To establish a causality relationship between exposure to endocrine disruptors and disease, experiments on animals must be performed with improved or new analytical tools. Therefore, a simple, rapid, and effective multi-residue method was developed for the determination of four steroid hormones (i.e., testosterone, androstenedione, estrone, and estradiol), glucuronide and sulfate conjugates of estrone and estradiol and four endocrine disruptors in rat testis (i.e., bisphenol A, atrazine, and active metabolites of methoxychlor and vinclozolin). The sample preparation procedure was based on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) approach. An analytical method was then developed to quantify these compounds at ultra-trace levels by liquid chromatography coupled to tandem mass spectrometry. The QuEChERS extraction was optimized with regard to the acetonitrile/water ratio used in the extraction step, the choice of the cleanup method and the acetonitrile/hexane ratio used in the cleanup step. The optimized extraction method exhibited recoveries between 89% and 108% for all tested compounds except the conjugates (31% to 58%). The detection limits of all compounds were below 20 ng g
−1
of wet weight of testis. The method was subsequently applied to determine the levels of hormones and EDCs in seven rat testis samples.
Figure
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| doi_str_mv | 10.1007/s00216-012-5723-2 |
| format | Article |
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−1
of wet weight of testis. The method was subsequently applied to determine the levels of hormones and EDCs in seven rat testis samples.
Figure
</description><identifier>ISSN: 1618-2642</identifier><identifier>EISSN: 1618-2650</identifier><identifier>DOI: 10.1007/s00216-012-5723-2</identifier><identifier>PMID: 22327963</identifier><language>eng</language><publisher>Berlin/Heidelberg: Springer-Verlag</publisher><subject>Acetonitrile ; Analytical Chemistry ; Animal behavior ; Animals ; Biochemistry ; Biochemistry, Molecular Biology ; Bisphenol A ; Characterization and Evaluation of Materials ; Chemical Fractionation - methods ; Chemical Sciences ; Chemicals ; Chemistry ; Chemistry and Materials Science ; Chromatography, Liquid - methods ; Cleaning ; Conjugates ; Drug Residues - analysis ; Drug Residues - isolation & purification ; Endocrine disruptors ; Endocrine Disruptors - analysis ; Endocrine Disruptors - isolation & purification ; Estrogen ; Extraction ; Food Science ; Herbicides ; Hormones ; Hormones - analysis ; Hormones - isolation & purification ; Humans ; Laboratory Medicine ; Life Sciences ; Male ; Mass spectrometry ; Mathematical analysis ; Monitoring/Environmental Analysis ; Original Paper ; Rats ; Rats, Sprague-Dawley ; Sulfates ; Tandem Mass Spectrometry - methods ; Testis - chemistry ; Testosterone</subject><ispartof>Analytical and bioanalytical chemistry, 2012-03, Vol.402 (9), p.2777-2788</ispartof><rights>Springer-Verlag 2012</rights><rights>COPYRIGHT 2012 Springer</rights><rights>Distributed under a Creative Commons Attribution 4.0 International License</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c576t-94f398072c93ac9ddcd72bf4dca44536973438c83750b1129a208f8f01d6b8f83</citedby><cites>FETCH-LOGICAL-c576t-94f398072c93ac9ddcd72bf4dca44536973438c83750b1129a208f8f01d6b8f83</cites><orcidid>0000-0002-5119-9801 ; 0000-0001-7271-9143</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://link.springer.com/content/pdf/10.1007/s00216-012-5723-2$$EPDF$$P50$$Gspringer$$H</linktopdf><linktohtml>$$Uhttps://link.springer.com/10.1007/s00216-012-5723-2$$EHTML$$P50$$Gspringer$$H</linktohtml><link.rule.ids>230,314,780,784,885,27924,27925,41488,42557,51319</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/22327963$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink><backlink>$$Uhttps://hal.science/hal-00727414$$DView record in HAL$$Hfree_for_read</backlink></links><search><creatorcontrib>Pouech, Charlène</creatorcontrib><creatorcontrib>Tournier, Mikaël</creatorcontrib><creatorcontrib>Quignot, Nadia</creatorcontrib><creatorcontrib>Kiss, Agneta</creatorcontrib><creatorcontrib>Wiest, Laure</creatorcontrib><creatorcontrib>Lafay, Florent</creatorcontrib><creatorcontrib>Flament-Waton, Marie-Magdeleine</creatorcontrib><creatorcontrib>Lemazurier, Emmanuel</creatorcontrib><creatorcontrib>Cren-Olivé, Cécile</creatorcontrib><title>Multi-residue analysis of free and conjugated hormones and endocrine disruptors in rat testis by QuEChERS-based extraction and LC-MS/MS</title><title>Analytical and bioanalytical chemistry</title><addtitle>Anal Bioanal Chem</addtitle><addtitle>Anal Bioanal Chem</addtitle><description>Endocrine disrupting compounds (EDCs) are suspected to be responsible for many disorders of the human reproductive system. To establish a causality relationship between exposure to endocrine disruptors and disease, experiments on animals must be performed with improved or new analytical tools. Therefore, a simple, rapid, and effective multi-residue method was developed for the determination of four steroid hormones (i.e., testosterone, androstenedione, estrone, and estradiol), glucuronide and sulfate conjugates of estrone and estradiol and four endocrine disruptors in rat testis (i.e., bisphenol A, atrazine, and active metabolites of methoxychlor and vinclozolin). The sample preparation procedure was based on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) approach. An analytical method was then developed to quantify these compounds at ultra-trace levels by liquid chromatography coupled to tandem mass spectrometry. The QuEChERS extraction was optimized with regard to the acetonitrile/water ratio used in the extraction step, the choice of the cleanup method and the acetonitrile/hexane ratio used in the cleanup step. The optimized extraction method exhibited recoveries between 89% and 108% for all tested compounds except the conjugates (31% to 58%). The detection limits of all compounds were below 20 ng g
−1
of wet weight of testis. The method was subsequently applied to determine the levels of hormones and EDCs in seven rat testis samples.
Figure
</description><subject>Acetonitrile</subject><subject>Analytical Chemistry</subject><subject>Animal behavior</subject><subject>Animals</subject><subject>Biochemistry</subject><subject>Biochemistry, Molecular Biology</subject><subject>Bisphenol A</subject><subject>Characterization and Evaluation of Materials</subject><subject>Chemical Fractionation - methods</subject><subject>Chemical Sciences</subject><subject>Chemicals</subject><subject>Chemistry</subject><subject>Chemistry and Materials Science</subject><subject>Chromatography, Liquid - methods</subject><subject>Cleaning</subject><subject>Conjugates</subject><subject>Drug Residues - analysis</subject><subject>Drug Residues - isolation & purification</subject><subject>Endocrine disruptors</subject><subject>Endocrine Disruptors - analysis</subject><subject>Endocrine Disruptors - isolation & purification</subject><subject>Estrogen</subject><subject>Extraction</subject><subject>Food Science</subject><subject>Herbicides</subject><subject>Hormones</subject><subject>Hormones - analysis</subject><subject>Hormones - isolation & purification</subject><subject>Humans</subject><subject>Laboratory Medicine</subject><subject>Life Sciences</subject><subject>Male</subject><subject>Mass spectrometry</subject><subject>Mathematical analysis</subject><subject>Monitoring/Environmental Analysis</subject><subject>Original Paper</subject><subject>Rats</subject><subject>Rats, Sprague-Dawley</subject><subject>Sulfates</subject><subject>Tandem Mass Spectrometry - methods</subject><subject>Testis - chemistry</subject><subject>Testosterone</subject><issn>1618-2642</issn><issn>1618-2650</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2012</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFks2O0zAUhSMEYoaBB2CDIrEYWGTG13ZsZ1lVhUFqhaCwthzbaV2lcbETRJ-A18aZDJWQ0FRe2Lr-7tH9OVn2GtANIMRvI0IYWIEAFyXHpMBPsktgIArMSvT09Kb4InsR4w4hKAWw59kFxgTzipHL7PdqaHtXBBudGWyuOtUeo4u5b_Im2DFgcu273bBRvTX51oe972y8j9vOeB1cZ3PjYhgOvQ8xd10eVJ_3NvZJpj7mX4bFfLv4ui5qFZOC_dUHpXvnu3uN5bxYrW9X65fZs0a10b56uK-y7x8W3-Z3xfLzx0_z2bLQJWd9UdGGVAJxrCuidGWMNhzXDTVaUVoSVnFCidCC8BLVALhSGIlGNAgMq9ODXGXvJ92tauUhuL0KR-mVk3ezpRxjaa6YU6A_IbHXE3sI_seQGpJ7F7VtW9VZP0RZjWMWgpFEvnuUBE4ph1QhnEcZB1IhlvZ5FsUYRFoo0PMoEgnmRIy1vp3QjWqtdF3jx4WMuJxRghAlFI1l3vyHSsfYvUuGsI1L8X8SYErQwccYbHOaLiA5ulVObpXJrXJ0qxwbfPNQ9VDvrTll_LVnAvAExPTVbWyQOz-E5NH4iOofQnzwCQ</recordid><startdate>20120301</startdate><enddate>20120301</enddate><creator>Pouech, Charlène</creator><creator>Tournier, Mikaël</creator><creator>Quignot, Nadia</creator><creator>Kiss, Agneta</creator><creator>Wiest, Laure</creator><creator>Lafay, Florent</creator><creator>Flament-Waton, Marie-Magdeleine</creator><creator>Lemazurier, Emmanuel</creator><creator>Cren-Olivé, Cécile</creator><general>Springer-Verlag</general><general>Springer</general><general>Springer Verlag</general><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7QH</scope><scope>7UA</scope><scope>C1K</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>L7M</scope><scope>7X8</scope><scope>1XC</scope><orcidid>https://orcid.org/0000-0002-5119-9801</orcidid><orcidid>https://orcid.org/0000-0001-7271-9143</orcidid></search><sort><creationdate>20120301</creationdate><title>Multi-residue analysis of free and conjugated hormones and endocrine disruptors in rat testis by QuEChERS-based extraction and LC-MS/MS</title><author>Pouech, Charlène ; Tournier, Mikaël ; Quignot, Nadia ; Kiss, Agneta ; Wiest, Laure ; Lafay, Florent ; Flament-Waton, Marie-Magdeleine ; Lemazurier, Emmanuel ; Cren-Olivé, Cécile</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c576t-94f398072c93ac9ddcd72bf4dca44536973438c83750b1129a208f8f01d6b8f83</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2012</creationdate><topic>Acetonitrile</topic><topic>Analytical Chemistry</topic><topic>Animal behavior</topic><topic>Animals</topic><topic>Biochemistry</topic><topic>Biochemistry, Molecular Biology</topic><topic>Bisphenol A</topic><topic>Characterization and Evaluation of Materials</topic><topic>Chemical Fractionation - methods</topic><topic>Chemical Sciences</topic><topic>Chemicals</topic><topic>Chemistry</topic><topic>Chemistry and Materials Science</topic><topic>Chromatography, Liquid - methods</topic><topic>Cleaning</topic><topic>Conjugates</topic><topic>Drug Residues - analysis</topic><topic>Drug Residues - isolation & purification</topic><topic>Endocrine disruptors</topic><topic>Endocrine Disruptors - analysis</topic><topic>Endocrine Disruptors - isolation & purification</topic><topic>Estrogen</topic><topic>Extraction</topic><topic>Food Science</topic><topic>Herbicides</topic><topic>Hormones</topic><topic>Hormones - analysis</topic><topic>Hormones - isolation & purification</topic><topic>Humans</topic><topic>Laboratory Medicine</topic><topic>Life Sciences</topic><topic>Male</topic><topic>Mass spectrometry</topic><topic>Mathematical analysis</topic><topic>Monitoring/Environmental Analysis</topic><topic>Original Paper</topic><topic>Rats</topic><topic>Rats, Sprague-Dawley</topic><topic>Sulfates</topic><topic>Tandem Mass Spectrometry - methods</topic><topic>Testis - chemistry</topic><topic>Testosterone</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Pouech, Charlène</creatorcontrib><creatorcontrib>Tournier, Mikaël</creatorcontrib><creatorcontrib>Quignot, Nadia</creatorcontrib><creatorcontrib>Kiss, Agneta</creatorcontrib><creatorcontrib>Wiest, Laure</creatorcontrib><creatorcontrib>Lafay, Florent</creatorcontrib><creatorcontrib>Flament-Waton, Marie-Magdeleine</creatorcontrib><creatorcontrib>Lemazurier, Emmanuel</creatorcontrib><creatorcontrib>Cren-Olivé, Cécile</creatorcontrib><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>Aqualine</collection><collection>Water Resources Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><collection>MEDLINE - Academic</collection><collection>Hyper Article en Ligne (HAL)</collection><jtitle>Analytical and bioanalytical chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Pouech, Charlène</au><au>Tournier, Mikaël</au><au>Quignot, Nadia</au><au>Kiss, Agneta</au><au>Wiest, Laure</au><au>Lafay, Florent</au><au>Flament-Waton, Marie-Magdeleine</au><au>Lemazurier, Emmanuel</au><au>Cren-Olivé, Cécile</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Multi-residue analysis of free and conjugated hormones and endocrine disruptors in rat testis by QuEChERS-based extraction and LC-MS/MS</atitle><jtitle>Analytical and bioanalytical chemistry</jtitle><stitle>Anal Bioanal Chem</stitle><addtitle>Anal Bioanal Chem</addtitle><date>2012-03-01</date><risdate>2012</risdate><volume>402</volume><issue>9</issue><spage>2777</spage><epage>2788</epage><pages>2777-2788</pages><issn>1618-2642</issn><eissn>1618-2650</eissn><abstract>Endocrine disrupting compounds (EDCs) are suspected to be responsible for many disorders of the human reproductive system. To establish a causality relationship between exposure to endocrine disruptors and disease, experiments on animals must be performed with improved or new analytical tools. Therefore, a simple, rapid, and effective multi-residue method was developed for the determination of four steroid hormones (i.e., testosterone, androstenedione, estrone, and estradiol), glucuronide and sulfate conjugates of estrone and estradiol and four endocrine disruptors in rat testis (i.e., bisphenol A, atrazine, and active metabolites of methoxychlor and vinclozolin). The sample preparation procedure was based on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) approach. An analytical method was then developed to quantify these compounds at ultra-trace levels by liquid chromatography coupled to tandem mass spectrometry. The QuEChERS extraction was optimized with regard to the acetonitrile/water ratio used in the extraction step, the choice of the cleanup method and the acetonitrile/hexane ratio used in the cleanup step. The optimized extraction method exhibited recoveries between 89% and 108% for all tested compounds except the conjugates (31% to 58%). The detection limits of all compounds were below 20 ng g
−1
of wet weight of testis. The method was subsequently applied to determine the levels of hormones and EDCs in seven rat testis samples.
Figure
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| subjects | Acetonitrile Analytical Chemistry Animal behavior Animals Biochemistry Biochemistry, Molecular Biology Bisphenol A Characterization and Evaluation of Materials Chemical Fractionation - methods Chemical Sciences Chemicals Chemistry Chemistry and Materials Science Chromatography, Liquid - methods Cleaning Conjugates Drug Residues - analysis Drug Residues - isolation & purification Endocrine disruptors Endocrine Disruptors - analysis Endocrine Disruptors - isolation & purification Estrogen Extraction Food Science Herbicides Hormones Hormones - analysis Hormones - isolation & purification Humans Laboratory Medicine Life Sciences Male Mass spectrometry Mathematical analysis Monitoring/Environmental Analysis Original Paper Rats Rats, Sprague-Dawley Sulfates Tandem Mass Spectrometry - methods Testis - chemistry Testosterone |
| title | Multi-residue analysis of free and conjugated hormones and endocrine disruptors in rat testis by QuEChERS-based extraction and LC-MS/MS |
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